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May | 2015

Sample preparation for chromatographic analysis of small molecules such as drugs and pesticides has evolved significantly over the past decade, becoming faster, more automated, and capable of extracting analytes for analysis at part-per-trillion and lower levels. This presentation will compare and contrast three approaches that have evolved most significantly. Solid-phase extraction is a classical technique that has received a recent high-tech boost from automation and miniaturization. Over the past decade, the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) approach provided a simple, low-tech alternative that has greatly impacted the analysis of pesticides and residues from numerous matrices, especially foods. Finally, multidimensional detection has led to a no-tech sample preparation approach in LC-MS analysis: none. Especially in multi-residue drug analysis from biological samples, methods involving no sample preparation at all are generating interest. The choice of approach depends on several chemical variables, including sample type, analytes, and desired analytical performance, plus managerial variables including cost, throughput and simplicity. Using examples drawn from the analysis of drug and pesticide residues in biological samples, these three approaches will be compared and contrasted with a view toward assisting laboratories in choosing or improving their own methods and techniques for these often difficult analyses.

HPLC for Pharmaceutical Analyses: Succeed with Sample Filtration

April | 2014

The entire pharmaceutical development workflow, from discovery to manufacturing and QC, relies heavily on HPLC and LC-MS analysis. Many chromatography challenges, such as poor peak resolution, poor run reproducibility, or short column life, can be traced back to improper sample preparation or mobile phase preparation. In this seminar, Vivek Joshi, PhD, of Merck reviews filtration as a sample prep technique and factors to consider while selecting appropriate filtration formats based on the stage within the pharmaceutical workflow. You will learn how to select appropriate high-throughput filtration systems commonly used in drug discovery, as well as considerations for lower-throughput approaches for manufacturing and QC operations. Dr. Joshi will also discuss tips and tricks for reducing extractables and nonspecific analyte binding. Then, Maricar Tarun-Dube, PhD, will explain the importance of ultrapure water quality in HPLC and LC–MS, demonstrating how contamination in reagent water can compromise analyses. Specifically, she will describe the challenges posed by particulates, bacteria, and organic molecules present in the mobile phase as well as strategies for overcoming these challenges.

Oct | 2013

Did you know that many challenges in chromatography analysis, such as distorted peaks, low signal-to-noise ratios, column failure, and baseline drift, can be prevented or reduced with careful consideration of sample preparation techniques and choosing the right materials? In this seminar, Dr. Vivek Joshi, of Merck, reviews filtration properties and chemical compatibility of different membrane materials. The importance of sample and mobile phase filtration prior to HPLC analysis will be discussed with supportive data. Tips and tricks for reducing extractables and nonspecific analyte binding also will be discussed. Moreover, throughput will be addressed, with recommendations for choosing sample preparation platforms based on number of samples and sample volume.